CN106929920A - The nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate - Google Patents
The nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate Download PDFInfo
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- CN106929920A CN106929920A CN201710077092.7A CN201710077092A CN106929920A CN 106929920 A CN106929920 A CN 106929920A CN 201710077092 A CN201710077092 A CN 201710077092A CN 106929920 A CN106929920 A CN 106929920A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
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Abstract
The invention provides a kind of CsPbBr based on thiocyanate doping3‑x(SCN)x(x=0,0.06,0.12,0.18) nanocrystalline preparation method of inorganic perovskite.Under conditions of inert gas shielding, first by PbBr2With Pb (SCN)2With reaction dissolvent octadecylene, surfactant oleic acid, oleyl amine mixing are completely dissolved it, then mixed solution is heated to reaction temperature, is then rapidly injected caesium presoma, system starts reaction generation perovskite structure, and with the carrying out of reaction, gradually form CsPbBr3‑x(SCN)xNanocrystalline, reaction quickly cools down product ice-water bath after terminating, that is, obtain final CsPbBr3‑x(SCN)xInorganic perovskite is nanocrystalline.The present invention, by doping Thiocyanate ion in various degree, on the premise of perovskite pattern and crystal structure is not changed, realizes the small regulation and control to inorganic perovskite optical property using heat injection synthetic method.Preferably, pattern is homogeneous, and the photoelectric device for constructing high-performance whole soln has far-reaching significance for the nanocrystalline monodispersity of perovskite and stability of synthesis.
Description
Technical field
The present invention relates to a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate, belong to new material system
Standby technical field.
Background technology
With the appearance of new perovskite solar cell, perovskite material is increasingly attracted attention by people, in recent years
Purely inorganic perovskite nano material is shown up prominently due to more excellent stability in photoelectric field.Inorganic perovskite nano material
With more excellent photoelectric properties, luminescent spectrum wider, photoelectric transformation efficiency higher and carrier mobility, response speed
Fast the advantages of, it is set to have in the fields such as solar cell, photodetector, optical pickocff, light emitting diode quite wide
Wealthy application prospect, Development volue is very high.
By ion exchange, inorganic perovskite ABX3Luminescent spectrum can realize in whole visible-range coordinate
(Akkerman,Q.A.；D'Innocenzo,V.；Accornero,S.；Scarpellini,A.；Petrozza,A.；Prato,
M.；Manna,L.,Tuning the Optical Properties of Cesium Lead Halide Perovskite
Nanocrystals by Anion Exchange Reactions.Journal of the American Chemical
Society 2015,137(32),10276-81.).At present, the method for regulation perovskite nano material optical property is mainly logical
Change X (Cl or Br or I adulterates two-by-two) is crossed come what is realized.But, this regulation and control method is carried out between halogen
Selection, research of the halogen to regulate and control optical property is substituted with the anion in addition to halogen and is not occurred still.The present invention is just
A kind of nanocrystalline synthesis technique of inorganic perovskite based on thiocyanate doping is there is provided, stable performance, pattern chi can be obtained
It is very little uniform and the nanocrystalline of small regulation and control can be carried out to its optical property.Therefore, realize that purely inorganic perovskite is nanocrystalline optical
The small regulation and control of energy have very profound significance for constructing the photoelectric device of high-performance whole soln.
The content of the invention
Technical problem：For problem of the prior art, there is provided a kind of inorganic perovskite nanometer based on doping thiocyanate
Brilliant preparation method, obtained all inorganic perovskites are nanocrystalline to be uniform cubic.By changing sulphur in the present invention
The doping of cyanogen root, make in perovskite cube-there is small deformation in octoploids structure, so as to realize the small tune of optical property
Control；On the other hand, the doping of micro thiocyanate can also increase the crystallinity of nano material.
Technical scheme：In order to solve the above-mentioned technical problem, the invention provides a kind of inorganic calcium based on doping thiocyanate
The nanocrystalline preparation method of titanium ore, comprises the following steps：
Step 1, during the precursor salt containing caesium is dissolved in into octadecylene, oleic acid, after vacuum drying, heating stirring makes it completely molten
Solution, is made into oleic acid caesium precursor solution, and this solution is used as storing solution；
Step 2, by reactant PbBr2、Pb(SCN)2Mixed solution is mixed to form with octadecylene, first the mixed solution is taken out
Vacuum, after be passed through inert gas, then vacuumize again, circulate operation；Last heat preservation and dryness under vacuum；
Step 3, is passed through inert gas, by surfactant oleic acid, the mixed solution of oleyl amine addition step 2, continues to protect
Temperature is completely dissolved reactant, and lead precursor solution is obtained；
Step 4, after obtained lead precursor solution is warming up into 150 DEG C, takes oleic acid caesium precursor solution in step 1, soon
Speed is injected into lead precursor solution, generates CsPbBr3-x(SCN)x；10s-60s is incubated at 145 DEG C -155 DEG C, then frozen water
The quick cooling of bath, that is, obtain CsPbBr3-x(SCN)xPerovskite is nanocrystalline.
Wherein：
In step 1, the described precursor salt containing caesium is cesium carbonate, and the molar concentration of described oleic acid caesium presoma is
0.125mol/L。
In step 1, described vacuum drying temperature is 110 DEG C -130 DEG C, and drying time is 1-2h.
In step 1, described heating-up temperature is 145 DEG C -155 DEG C, and the heat time is 1-2h, and mixing speed is 900-
1000rpm。
In step 2, described PbBr2、Pb(SCN)2Total material amount be 0.188mmol, Pb (SCN)2Account for total material
The ratio of amount is 0.1%-6%；Mixing speed is 900-1000rpm.
In step 2, described circulate operation number of times is 3 times, and holding temperature is 110 DEG C -130 DEG C, and soaking time is 1-2h.
In step 3, the oleic acid of the addition, the volume ratio of oleyl amine are 1:1, and be after 60 DEG C are vacuum dried 0.5h
Anhydrous solvent.
In step 4, the oleic acid caesium presoma storing solution of described addition must be previously heated to 95 DEG C -105 DEG C；With lead forerunner
The volume ratio of body is 1:(12-13)
In step 4, the CsPbBr for obtaining3-x(SCN)xIt is 1 that nano whisker adds volume ratio:The tert-butyl alcohol of (1-2) is made
It is precipitating reagent, then centrifugation.
Beneficial effect：It is an advantage of the invention that：1) the nanocrystalline monodispersity of inorganic perovskite and stabilization of present invention synthesis
Property preferably, pattern is homogeneous；2) raw material needed for perovskite synthesis are simple, and technology of preparing stabilization, method is simple, easy to operate,
Repetitive rate is high；3) hot injection method can make nanocrystalline crystallinity more preferably, excellent in optical properties.By the doping for changing thiocyanate
Amount, can send the fluorescence of adjustable 514nm-496nm, and ultraviolet-ray visible absorbing also occurs corresponding blue shift, is conducive to the later stage
The regulation of photoelectric device performance.
Brief description of the drawings
Fig. 1 is the nanocrystalline TEM figures of inorganic perovskite obtained in embodiment 1-4；
Fig. 2 is the nanocrystalline XRD of inorganic perovskite obtained in embodiment 1-4 and standard diagram (JCPDS：54-0752)
Contrast；
Fig. 3 is the nanocrystalline UV absorption and fluorescence emission spectrogram of compound of inorganic perovskite obtained in embodiment 1-4.
Specific embodiment
The present invention is further described with reference to embodiment and accompanying drawing.
The nanocrystalline preparation method of inorganic perovskite of the present invention based on doping thiocyanate, is the bar in inert gas shielding
Under part, first by PbBr2With Pb (SCN)2With reaction dissolvent octadecylene, surfactant oleic acid, oleyl amine mix and make it completely molten
Solution, is then heated to reaction temperature by mixed solution, is then rapidly injected caesium presoma, and system starts reaction generation perovskite knot
Structure, and with the carrying out of reaction, gradually form CsPbBr3-x(SCN)xIt is nanocrystalline, react the fast quickly cooling of product ice bath after terminating
But, that is, final CsPbBr is obtained3-x(SCN)xInorganic perovskite is nanocrystalline.
Embodiment 1：
Step 1, by 2.5mmol Cs2CO3It is dissolved in 40ml octadecylenes, 2.5ml oleic acid, after 120 DEG C of vacuum drying 1h, leads to
Enter nitrogen, being warming up to 150 DEG C is completely dissolved it, form oleic acid caesium precursor solution, this solution is used as storing solution；
Step 2, by 0.0690g PbBr2、0g Pb(SCN)2Mix with octadecylene, first vacuumize mixed solution, lead to afterwards
Enter inert gas, then vacuumize again, circulate operation 3 times；Last 120 DEG C of heat preservation and dryness 1h under vacuum；
Step 3, is passed through inert nitrogen gas, and surfactant 0.5ml oleic acid, 0.5ml oleyl amines are separately added into step 2
In mixed solution, continuing insulation is completely dissolved reactant, and lead precursor solution is obtained；
Step 4, after being warming up to 150 DEG C, takes oleic acid caesium precursor solution 0.4ml in step 1, is rapidly injected step 3
In lead precursor solution, CsPbBr is generated3；10s-60s is incubated at 150 DEG C, then ice-water bath is quickly cooled down, that is, obtain
CsPbBr3Perovskite is nanocrystalline.
Step 5, adds the tert-butyl alcohol as precipitating reagent, and 5min is centrifuged through 7000rpm, removes supernatant.Precipitation is taken to be dissolved in
CsPbBr is can obtain in n-hexane3Nanocrystalline dispersion liquid.
Example 2：
Using the same process of embodiment 1, difference is, 2 the step of by embodiment 1) in PbBr2、Pb(SCN)2Quality point
0.0676g, 0.0012g are not changed to, other conditions are consistent, the product for obtaining is CsPbBr2.94(SCN)0.06。
Example 3：
Using the same process of embodiment 1, difference is, 2 the step of by embodiment 1) in PbBr2、Pb(SCN)2Quality point
0.0662g, 0.0024g are not changed to, other conditions are consistent, the product for obtaining is CsPbBr2.88(SCN)0.12。
Example 4：
Using the same process of embodiment 1, difference is, 2 the step of by embodiment 1) in PbBr2、Pb(SCN)2Quality point
0.0649g, 0.0036g are not changed to, other conditions are consistent, the product for obtaining is CsPbBr2.82(SCN)0.18。
By adjusting thiocyanate doping, can to obtain homogeneous pattern, good dispersion, stability perovskite high nanocrystalline,
With increasing for doping, can be seen that its pattern, size and lattice structure from Fig. 1,2 and be basically unchanged, keep original inorganic calcium
Titanium ore it is good cube-octahedral structure.UV-Vis spectrum and fluorescent emission collection of illustrative plates in comparison diagram 3, find with the increasing of doping
Plus, absorbing and transmitting collection of illustrative plates occurs certain blue shift, its fluorescence emission peak is respectively 514nm, 508nm, 506nm,
496nm。
Claims (9)
1. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate, it is characterised in that the preparation method bag
Include and comprise the following steps that：
Step 1, during the precursor salt containing caesium is dissolved in into octadecylene, oleic acid, after vacuum drying, heating stirring is completely dissolved it, matches somebody with somebody
Into oleic acid caesium precursor solution, this solution is used as storing solution；
Step 2, by reactant PbBr2、Pb(SCN)2Mixed solution is mixed to form with octadecylene, first the mixed solution is vacuumized,
After be passed through inert gas, then vacuumize again, circulate operation；Last heat preservation and dryness under vacuum；
Step 3, is passed through inert gas, and by surfactant oleic acid, the mixed solution of oleyl amine addition step 2, continuing insulation makes
Reactant is completely dissolved, and lead precursor solution is obtained；
Step 4, after obtained lead precursor solution is warming up into 150 DEG C, takes oleic acid caesium precursor solution in step 1, quick note
Enter in lead precursor solution, generate CsPbBr3-x(SCN)x；10s-60s is incubated at 145 DEG C -155 DEG C, then ice-water bath is fast
Quickly cooling but, that is, obtains CsPbBr3-x(SCN)xPerovskite is nanocrystalline.
2. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is that in step 1, the described precursor salt containing caesium is cesium carbonate, and the molar concentration of described oleic acid caesium presoma is
0.125mol/L。
3. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is that in step 1, described vacuum drying temperature is 110 DEG C -130 DEG C, and drying time is 1-2h.
4. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is that in step 1, described heating-up temperature is 145 DEG C -155 DEG C, and the heat time is 1-2h, and mixing speed is 900-
1000rpm。
5. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is, in step 2, described PbBr2、Pb(SCN)2Total material amount be 0.188mmol, Pb (SCN)2Account for the amount of total material
Ratio be 0.1%-6%；Mixing speed is 900-1000rpm.
6. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is that in step 2, described circulate operation number of times is 3 times, and holding temperature is 110 DEG C -130 DEG C, and soaking time is 1-2h.
7. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is that in step 3, the oleic acid of the addition, the volume ratio of oleyl amine are 1:1, and be after 60 DEG C are vacuum dried 0.5h
Anhydrous solvent.
8. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is that in step 4, the oleic acid caesium presoma storing solution of described addition must be previously heated to 95 DEG C -105 DEG C；With lead presoma
Volume ratio be 1:(12-13).
9. a kind of nanocrystalline preparation method of inorganic perovskite based on doping thiocyanate as claimed in claim 1, its feature
It is, in step 4, the CsPbBr for obtaining3-x(SCN)xIt is 1 that nano whisker adds volume ratio:The tert-butyl alcohol conduct of (1-2)
Precipitating reagent, then centrifugation.
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| CN114657628A (en) * | 2022-02-28 | 2022-06-24 | 电子科技大学 | Method for preparing perovskite nanocrystalline by double-source organic lead source |
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